Seed-meal glue



Patented Feb. 23, 1943 The Borden Company, New York, N. Y., a corporation of New Jersey No Drawing.

Application November 27, 1939, [Serial No. 306,411

6Claims. (01. 106-154) a "This invention has for its object to 'improve thewaterresistance properties of glues containing seedmeal as a component. The art of manufacture and use of seedmeals, especially for the gluing of laminated wood, paper and the like, is well known and does not need a detailed review. In brief, various high protein seedmeals such as soya, peanut, cottonseed and the like, preferably from which the greater portion of the oils have been expressed or otherwise removed, are finely ground, preferably to practically all pass a 200 mesh screen, and the resulting fine meal is mixed with various chemicals, for example alkaline salts, and/or caustic alkali, hydrated lime, etc., and with water to produce a glue. Very large glues are largely used in the gluing of plywood and-inaddition-td the seedmeal, may contain casein, I or not, as'desired.

A'great variety of formulas have been suggested as regards the chemicals added for making above mentioned formulas give a very good dry strength. But test samples of the glued up plywood, testedafter soaking in water for 48 hours, (and'without again drying) according to standard specifications, e. g. on the well known Riehle .quantities of such glues are used annually. Such testing machine, show results that are often too this lack of water resistance on the glued panels and in some instances with more or less success. For instance it has'been suggested that various amounts of carbon'bisulphide be added to the liquid glue in order to increase the water resistance." Others have suggested the use of a mixture of carbon bisulphide and formaldehyde, etc. In any of these suggested processes so far as I am aware, there are objectionable features. Carbon bisulphide is poisonous and is a serious objegtion in gnill practice since the fumes of the carbon bisulphide are known to be dangerous for workmen .;to breathe. It is also extremely inflammable and explosive, and has an objectionable odor.

- During a long search ance on seedmeal glues for gluing wood and the like, I have found that under proper conditions, I' obtain very good results at a low cost and without any industrial hazards, by the use of rela-' tively small amounts of sulphonated oils with seedmeal glues, and I have demonstrated that particularly satisfactory results are obtainable when using sulphonated oils with soluble copper salts, such as copper sulphate. I am aware that copper sulphate or other water soluble copper salts ha been proposed in the past for the improvement of water resistance in protein glues including seedmeal glues, but my research has thoroughly proven the fact that the use of a water soluble copper salt such as copper sulphate in seedmeal glues does not give the same degree of water resistance which can be obtained when using a mixture of copper sulphate and sulphonated oils in the glue.

In order to more fully disclose my invention, I give below a series of tests showing the results from gluing fir panels with a seedmeal glue without copper sulphate or sulphonated oil; another series showing the strength, wet and,dry, of the same glue with copper sulphate alone; a third series using the same glue but with an addition of both copper sulphate and sulphonated oil and a fourth series showing tests with sulphonated oil with no addition of copper sulphate. As I have indicated above, there are many possible combinations of chemicals or protein solvents that may be used in making a seedmeal glue and .the example I give below is simply one of many such combinations and is only given by way ofexample.

The glue base mixture used in the following tests was prepared as follows:

' Pounds Finely ground soybean 'meal (substantially all passing through a standard 200 mesh wire sieve '49 Finely ground cottonseed meal (substantially all passing a standard 200 mesh wire sieve Trisodium phosphate (of the usual commercial quality 2 The meals referred to were made from presscakes which were substantially free from oil, and

are the commercial grades used in glue manufacture.

- glue.

To the lbs. of dry material referred to above, I prefer to add 2 lbs. of kerosene oil of any ordinary commercial grade. For this purpose, the entire dry materials are thoroughly mixed together and thereafter 2 lbs. of kerosene oil is poured or'sprayed onto the mass and it is thoroughly mixed in order to get the kerosene oil thoroughly and uniformly mixed with the! In instances where reference is made to the use of copper sulphate in any of these tests the amount of copper sulphate in a finely ground condition of about 80 mesh or finer, is also added to the dry components of the glue mix, and uniformly incorporated therein. This glue base either with or without the copper sulphate was prepared for application to wood in making 3 ply veneer panels, as follows (all parts by weight):

300 parts of-cold water (i. e. tap water as drawn from the town water supply), are placed in a suitable kettle with an agitator preferably running at 360 R. P. M. Thereafter, 100 parts of the dry glue base is sifted into the mixer containing the cold water and thoroughly mixed for about 2 minutes. Thereafter, 10 parts of very finely ground commercial hydrated lime, preferably already mixed with25 lbs. of cold water, is added to the mix and the mixing continued for about 3 minutes. I then added .7 parts of commercial caustic soda preferably already dissolved in 15 parts of water and. continued to mix for 4 minutes. Thereafter, 25 parts of commercial sodium silicate solution, preferably of the type known as N grade, about 41 B., was added and the mixing continued for 5 minutes. I then added 40 parts more of cold water and mixed about 3 minutes, when the glue is ready for use. This represents theaglue without either the sulphonated oil or the copper sulphate.

In the tests wherein I use both sulphonated oil and copper sulphate, the same dry glue base plus' glue was followed with the exception that after the addition of the silicate of soda or immediately after the silicate of soda is mixed into the glue, I added 2 parts of sulphonated oil,' In the tests where sulphonated oil and no copper sulphate was used the same procedure was followed but no copper sulphate added to the dry glue.

Semi-commercial gluing tests were made by the general method. described above. Series A bein made with the glue alone, i. e. without the use of copper sulphate or sulphonated oil; series Bwith the use of the glue with copper sulphate but without the sulphonated oil, and series C with the use of the glue with sulphonated oil but without copper sulphate, and Series D with the use of the glue with both the copper sulphate and the sulphonated oil. The resulting glues of these series were placed in a semi-commercial glue spreading machine such as is used in the industry. 1 6" thickness fir veneer were used in all the tests here reported, and 3-ply panels were made, using a spread in each case on the basis of 24 lbs. of

the dry glue per 1000 sq. ft. of double glue line.

That is to say on 1000 sq. ft. finished 3-ply fir panels there had been used in each instance, 24 lbs. of dry glue per 1000 sq. ft. to obtain the bond. All this plywood was pressed at 150 lbs. per sq. in.

The glued panels were allowed to stand under the pressure for about 12 hours; they were then removed and allowed to season for 5 days at ordinary room temperature and thereafter test strips were cut from the panels and tests were made on a Riehle testing machine for dry strengths, and another series of these strips were tested by soaking the test strips in cold water for 48 hours and thereafter immediately tested for wet strength. The resulting strength tests (wet and dry) which indicate pounds per square inch to cause the break, are shown in the following table:

Mean

Dry Wet Series A-Straight glue, no waterproofing agent 264-2; 100-0 Series B-Glue plus 2% Cu sulphate, no sulphonited oil 242-18 112-0 Series Glue plus 2% sulphonated neats-ioot 011.. 240-47 116-0 Glue plus 2% sulphonated mineral oil. 233-30 115-0 Glue plus 2% sulphonated cottonseed 011.. 320-47 132-2 8 *rles D- L Glue plus 2% CuSOH-sulpbonated neat'sfoot oil 250-23 125-0 Glue plus 2% CnSOt+su1phonated minoi f a e-s6 i-"ul Ii tH tt 242-28 12H ue us u s one e 00 onsee oiluf .5 326-71 191-12 In the series showing wet and dry strengths, A, B, C and D, there will be noted a figure immediately after the first number, the figure separated by a hyphen. This second set of figures under both dry and wet columns represents the percentage of broken fibre that appears on the broken test piece. If on the other hand there was no broken fibre developed then the figure opposite the strength is represented by zero. As an example, under series AI found a dry strength of 264 lbs. and a fibre raise of 23%. Whereas in the same series under the wet strength, I found 100 lbs. wet strength and no fibre raise, represented by zero.

Under series C and D, it will be noted that tests were made (in this series) with various sulphonated oils, namely sulphonated neats-foot oil, which was in this case a 60% sulphonation; a

sulphonated cottonseed oil which was a 75% sulphonation, and a sulphonated mineral oil which was between and sulphonation.

As will be noted from these tests the most effective type of sulphonated oil either when used alone in the glue, or with copper sulphate, was obtained with sulphonated cottonseed 011, al-

though the tests made with the other sulphonated sulphonated oils for the purpose of this specificstion, I mean any type of sulphonated animal oil, vegetable oil or mineral oil. Neither do I wish to limit the percentage of sulphonated oils or copper sulphate that may be used.

In my tests I have noted in some cases that the water resistance of the wood panel is increased somewhat when larger amounts-of sulphonated oil are used and I therefore, do not wish to limit my invention to any stated percentage. I have Parts Casein 60 Cottonseed meal 29 Finely ground wood fiour 5 Trisodium phosphate 3 Sodium fluoride 3 These various materials are thoroughly blended together in' a mixer in the dry condition and a series of 4 gluing tests made as follows:

1. 250 parts of cold water were placed in a suitable mixer with a stirrer and to this cold water was added 100 parts of the above mentioned blend glue mixture. The stirring was continued for minutes and thereafter parts of finely ground hydrated lime, preferably mixed with 25 parts of cold water, was added and the mix stirred for another 5 minutes. Thereafter, 20 parts of silicate of soda N grade was added, continuing the stirring for another 5 minutes and finally parts of cold water added and the mixture stirred for another 3 minutes.

2. Same procedure as in No. 1 with the exception that 2 parts of sulphonated castor oil were added and stirred into the mixture just prior to the addition of the final 15 parts of diluting water.

3. Same procedure as in No. l'with the exception that 2 parts of powdered copper sulphate were added to the dry base mixture.

4. Same as in' example No. 1 with the exception that 2 parts by weight of powdered copper sulphate were added to 98 parts of the dry base glue mixture and 2 parts by weight of 75% sulphonated castor oil were added to the mixture just prior to the final addition of the 15 parts of diluting water.

These resulting glue mixtures series 1 to. 4 inclusive, were spread on 1 6 fir veneer 3-ply panels and were spread at the rate of 28.8 lbs. of the dry glue to every 1000 sq. ft. of double glue line. That is to say, it took 28.8 lbs. of the dry glue mix to make 1000 sq. ft. of the finished 3-ply panels. The glued veneers were pressed in a hydraulic press at 150 lbs. per sq. in., allowed to remain under pressure for 12 hours, removed and allowed to season for 5 days and thereafter strips cut from these panels were tested in the usual manner for dry and wet strengths. An average of these strength tests were as follows:

Dry Fibre Wet Fibre strength raised strength" raised ous types of high protein seedmeals and mixtures of these, and different salts can be used.

Thus, I have obtained excellent results when using a portion of blood albumin or dried blood in glues prepared according to this invention. For instance in certain tests I substituted 5% of spray dried blood albumin in place of 5% of seedmeal in a formula similar to the above and proceeded in preparing the glue and makinggluing tests and wet and dry strength tests, and

obtained excellent results; Other tests were also made with larger amounts (10% or more) of dried blood or blood albumin with satisfactory results. Furthermore, it is of course well under- 5 stood that various fillers may be added to these glues if desired, such as finely ground wood flour, or finely ground nut shells, or other desired filling material.

Obviously this invention also is not limited to 10 cold pressing but any improved glue composition within the scope of the appended claims may be used and hot'plate pressing may be used if desired. Furthermore, the invention is not restricted to the use of cold water for mixing the liquid 15 glue, nor to the use of particular alkalies (e. g. the trisodium phosphate and silicate of soda, given in the examples).

I have referred above to adding the sulphonate oil and the copper salt during dissolving. If desired, the sulphonated oil can be sprayed upon the dry mixed glue or partly mixed dry glue or upon the .seedmeal, to give a uniform mixture.

The copper salt if used, can be mixed with the dry glue or with the dry seedmeal.

I have referred above to the N grade" of sodium silicate. This is a syrupy liquid of 41 B., containing about 28.7% S102 and about 8.9%

Na'zO. Other syrupy solutions of sodium silicate can be employed, in equivalent quantity.

I claim:

1. A glue suitable for use in making plywood A containing a seedmeal of high protein content,

an alkali, a water soluble copper salt and a sulphonated oil in amount suflicient to substantially increase the wet strength.

2. A glue suitable for use in making plywood containing a. seedmeal of high protein content, casein, an alkali, a water soluble copper salt and a sulphonated oil, both of which are present in such amounts as to increase the wet strength of plywood glued up with said glue.

3. The step of adding a water soluble copper salt and asulphonated oil during the making of a fluid spreadable plywood glue containing seedmeal of high protein content, the amount of said sulphonated oil being suflicient to substantially increase the wet strength.

4. The step of adding a soluble copper salt and a sulphonated oil during the making of a fluid spreadable glue containing seedmeal of high protein content, and containing casein, the amount of said sulphonated oil being "sufficient to substantially increase the wet strength.

5. A glue suitable for use in making plywood containing a seedmeal of high protein content and an alkali, a small percentage of a watersoluble copper salt and about 2% of a sulphonated oil, based on the weight of the dry glue.

6. A glue suitable for use in making plywood containing a seedmeal of high protein content and an alkali, about 2% of a water-soluble copper salt and about 2% of a sulphonated oil, the percentages being based on the weight of the dry glue.

DONALD J. WHITE. 

